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Sulfuric Acid → 2,5-Dichloro-4-sulfanylphenol

HRID 858146
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HRID 858146 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([OH:8])[C:5]([Cl:9])=[CH:4][C:3]=1[S:10](Cl)(=O)=O.OS(O)(=O)=O>[Zn].C1(C)C=CC=CC=1>[Cl:9][C:5]1[CH:4]=[C:3]([SH:10])[C:2]([Cl:1])=[CH:7][C:6]=1[OH:8]
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참가 물질

5

반응물 2

HCID 1118Sulfuric AcidHCID 12526986HCID 12526986, 화합물

생성물 1

HCID 695140652,5-Dichloro-4-sulfanylphenol수율 54%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 1140Toluene용매

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온도
120 °C

실험 절차

To a mixture of 2,5-dichloro-4-hydroxy-benzenesulfonyl chloride (1.28 g, 4.92 mmol) and a solution of 25% of H2SO4 (17 mL), Zinc dust (1.64 g, 24.56 mmol) was added slowly at room temperature. The reaction mixture was allowed to stir at 120° C. overnight. The mixture was then cooled at room temperature and toluene was added. The layers were separated and the aqueous phase was dried over, MgSO4 filtered and concentrated in vacuo to give 514 mg (54%) of the title compound as a white solid, which was used in the next reaction without further purification.

후처리

  1. temperatureThe mixture was then cooled at room temperature
  2. customThe layers were separated
  3. dry with materialthe aqueous phase was dried over, MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-97109a784b9c43949ddb48c4d4df10b4
출처 데이터셋
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07148236B2

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